The epitaxial growth of Fe
1−xS formed on the (110) and (100) faces of Fe single crystals in H
2S-H
2 gas mixture at elevated temperature was investigated by electron diffraction and X-ray diffraction. Sulfidation was carried out at 250°C to 700°C for 1 to 15 min in 700 ppm H
2S.
The initial stage of scale growth was observed by means of a transmission electron microscope and a scanning electron microscope. The main results obtained are as follows:
(1) The epitaxial relationship between Fe
1−xS single crystal and Fe single crystal is independent of the crystal face of the substrate and (0001)Fe
1−xS is parallel to the substrate surface.
(2) Fe
1−xS single crystal is ordered FeS like troilite. The lattice constant of the Fe
1−xS crystal measured by electron diffraction is found to decrease with sulfidation temperature; 5.40 Å at 700°C and 5.96 Å at 250°C.
(3) The lattice constant of the Fe
1−xS crystal approaches an equilibrium value with annealing in H
2. As the sulfide crystal lattice has some geometical misfit, minimum −1.42% for the Fe lattice, it is concluded that small anisotropic strains caused by the epitaxial force between sulfide and substrate lattices exist in the sulfide scale. The strains measured after annealing are about −1% and compared with calculated result derived from Van Der Merwe’s expression.
(4) The initial stage of the double layer structure obtained by sulfidation of H
2S was observed by transmission and scanning electron microscopes. Thus, the scale formation mechanism is considered to occur by quasi-sintering with condensation of cation vacancies of the Fe
1−xS lattice occupied by hydrogen ions.
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